Wang Lu, Zang Xiaohuan, Wang Chun, Wang Zhi
Department of Chemistry, College of Science, Agricultural University of Hebei, Hebei, China.
J Sep Sci. 2014 Jul;37(13):1656-62. doi: 10.1002/jssc.201400028. Epub 2014 May 12.
A simple hydrophilic polyamide organic membrane protected micro-solid-phase extraction method with graphene oxide as the sorbent was developed for the enrichment of some parabens from water and vinegar samples prior to gas chromatography with mass spectrometry detection. The main experimental parameters affecting the extraction efficiencies, such as the type and amount of the sorbent, extraction time, stirring rate, salt addition, sample solution pH and desorption conditions, were investigated. Under the optimized experimental conditions, the method showed a good linearity in the range of 0.1-100.0 ng/mL for water samples and 0.5-100.0 ng/mL for vinegar samples, with the correlation coefficients varying from 0.9978 to 0.9997. The limits of detection (S/N = 3) of the method were in the range of 0.005-0.010 ng/mL for water samples and 0.01-0.05 ng/mL for vinegar samples, respectively. The recoveries of the method for the analytes at spiking levels of 5.0 and 70.0 ng/mL were between 84.6 and 106.4% with the relative standard deviations varying from 4.2 to 9.5%. The results indicated that the developed method could be a practical approach for the determination of paraben residues in water and vinegar samples.
建立了一种以氧化石墨烯为吸附剂的简单亲水性聚酰胺有机膜保护的微固相萃取方法,用于在气相色谱-质谱检测之前从水和醋样品中富集某些对羟基苯甲酸酯。研究了影响萃取效率的主要实验参数,如吸附剂的类型和用量、萃取时间、搅拌速率、加盐量、样品溶液pH值和解吸条件。在优化的实验条件下,该方法对水样在0.1 - 100.0 ng/mL范围内以及对醋样在0.5 - 100.0 ng/mL范围内均呈现良好的线性,相关系数在0.9978至0.9997之间。该方法对水样的检测限(S/N = 3)在0.005 - 0.010 ng/mL范围内,对醋样的检测限在0.01 - 0.05 ng/mL范围内。在加标水平为5.0和70.0 ng/mL时,该方法对分析物的回收率在84.6%至106.4%之间,相对标准偏差在4.2%至9.5%之间。结果表明,所建立的方法可为测定水和醋样品中对羟基苯甲酸酯残留提供一种实用的方法。